Process of treating ores.



P. A. EMANUEL.

PROCESS OF TREATING 032s.

Patented May 10, i910.

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- APPLICATION FILED SEPT 29, 1909 95573755.. I

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P. A. EMANUEL.

PROCESS OF TREATING ORES.

APPLICATION 31mm SEPT. 29, 1909.

I 957,755., Patented Ma 10, 1910.

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PHILIP A. EMANUEL, or AIKEN, SOUTH CAROLINA.

' rnocnss or TREATING oans;

. V r\ To all wit-om t1 may concern:

Be it known that I, PHILIPA. EMANUEL,

a citizen of the United States, residing at Aiken, in the. county of Aiken and State of South Carolina, have. invented certain new and useful Improvements in Processes of Treating Ores; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same. My invention relates to processes of treating ores and is designed to treat ordinary claysin such a manner as to save all their, valuable constituents'and at the same time make use of the by-products. It is also applicable to the treatment of bauxite and corundum for the making of soda, a double sulfate of sodium and aluminum, silica, aluminum fluorid, sodium sulfate, metallic sodium, and aluminate of sodium.

I carry out my process by an apparatus a part of which is shown in the accompanying dawings, and in which- Figure l is a side elevation showing my invention. Fig. 2 is'a horizontal cross section thereof. Fig. 3 is a cross section through the retort. Fig. 4 is a side elevation 'on a larger scale, showing part of the retort and part of the furnace, and Fig. 5 is a partial section showlng part of the retort and the drical, and open at both ends, but having one end bent inwardly to embrace the portion 2, both ends of the retort being exactly similar.

4 represents a perforated plate fitting tightly against the end of the retort, a suit- I able packing 50f asbestos or similar material being used if desired. Bolts 6 pass through the bent-in end of the part 3 through the part 2 and through the plate 4, uniting the whole firmly together.

7 represent tgbes whlch pass through the end plates 4, the ends of which are secured in perforations in the plate 8, secured to the plate 4. i

At the top and bottom the retort is pro- Specification oi Letters Patent.

- of the Patented May 10, 1910, Application filed Septemberfil-J, 1909. Serial No. 520,214.

vided with curved doors 9, hinged thereto,

and with two pipes 10, each provided with a .ock, such as 11, screwed. into the cover. Each of the doors is mounted on a rod 12,

in ears 13, projecting from the body of the retort-,and on the retort are mounted swingingbolts 14, adapted to swing down behind projections 15 on the cover, thus firmly I locking the covers in position. Any desired means, however, may be adopted for fastenheld in place by, the wire netting 15, the Z1 ends of said netting opposite the cover portion being secured to the rods 12 by having the ends of the wires wrapped around it,

as shown at 16.

The retort is thickened 'atthc center, and fromthese thickened portions run shafts 17, one of which is provided with a pulley 18, to which power may be applied to rotate the retort, as hereinafter described. Ordinarily, the retort is suspended from a triangular frame 19,- by means of depending supports 20 therefrom, terminating in bearings 21, engaging the rods 17. When it is desired to move the retort, the lower half of each bearing is removed.

To hold the parts A, B and C firmly bound together, in case the bearings 20 are moved, I provide two stout' upwardly-extending brackets 22, a little below the center of the outside of the parts 3. These brackets are firmly fastened to the parts 3 by being bolted thereto, or made integral therewith, and have their upper parts bent outwardly for engagement with the latches hereinafter mentioned. With each of the brackets 22 a pivoted latch is adapted to engage, two of these latches being pivotally mounted on the part B, and two on the part C. Each latch 23 has its end thickened, as

shown at 24, to pass down around the corresponding bracket 22, so that' when the latches are in the position shown in Fig. 1, thef-parts A, B and C areprevented from longitudinal movement, except as a whole, being firmly locked together, with the ends arts 3 fitting into corres onding grooves in the parts B and C. To t e parts B and Care-attached wheels 25, inthe usual manner, which are adapted to run on tracks 26, so that the whole apparatus, consisting of the parts A, B and C may be moved as a -who1e from one part of the plant to another, the latches being in the position shown in Fig. l, or whereby when the latches 23 are thrown up, the parts B and C may be separated from the retort A, whereupon the latter may be rotated by means of power applied to the pulley 18 for a purpose hereinafter described. The part B is the furnace portion, and is provided with a grate 26, pipe 27 for the admission of gaseous or liquid fuel, and door 28, provided with a latch 29., Of course, any desired form of fuel could be used in the part B.

The rear end of the part B is closed by a perforated plate 30, the perforations being located opposite the tubes 7 in the retort A. Around thls perforated plate, the rear open end of the part B is thickened, as shown at 31, and is provided with a circular groove,

into which groove the part 3 carried by the retort is adapted to fit. p The part G simply serves to carry the waste products of combustion after they have passed through the tubes 7 of*the retort into the chimney. It consists of a flue,

preferably cylindrical in form, having one end thickened, as shown at 32, said thickened end having a groove therein for the 30 reception of retort A.

33 represents a chimney, and 34; the flue thereof.

35 represents a cylindrical o ening, into which the open end of the part is adapted to telescope. This arrangement is adopted so that the parts'B and C maybe moved along the track out of engagement with the retort A, leavin the latter free to rotate.

The 0 eration is as follows :,The apparatus being in the position shown in Fig. 1, if it is desired to make gas, coke, and gas retort carbon, for example, the upper door of the retort is opened and a suitable charge of soft coal introduced into the interior of said retort into the space between the pipes 7. The upper door is then firmly closed, and connections made between the discharge pipes 10 at the top of the retort leading to the gasometer, or to any place Where gas is to be used. A fire is then started in the furnace B, and the hot products of combustion pass through the tubes 7, distilling the coal in the retort A, the gases passing out through the discharge pipes 10. After this operation has been continued for a sufficient tlmeto distil about half of the coal, the latches 23 are disengaged from the brackets 22, and the parts Band C moved along the track 26 out of contact with the retort'A. All the cooks in the pipes 10 bein closed, theu per pipes are disconnected om the pipes eading to the gasometer, and by means of power applied to the tort is rotated 180?. The parts B and C he part 3 on one end of the pulley 18, the i eare then brought back into connection with the retort A, and the latches 23 moved down into the position shown in Fig. 1. [he pipes at the top of the retort are then connected to the gas delivery pipes, and the cocks therein opened. The distillation process is therg carried on to its close, and at the end the upper pipes are disconnected from the as delivery pipes, andlboth the upper and ower doors are opened. By means of iron rods, the coke between the pipe 7 is forced down, out through the lower door, leaving the ipes 7, and in fact the Whole interior of t e retort, coated with an even layer of gas carbon.

. The fact that the whole intericrof the retort, including the pi es, is coated with an even layer of gas car on, makes the retort highly useful in the production-of sodium, for example, in which it is necessary that the substances under treatment should be subjected to the action of carbon under heat, and inwhich it is desirable that the retort should be frequently rotated. These retorts may be used either 'with or without carbon amount of carbon in the retort and for other reactions there must be no carbon. To obtain this carbon, I charge the retort with soft coal and heat the same, up to the'distillation point, by burning gas, coke, coal, or any desired kind of fuel in the furnace B. As the retort A becomes heated up, the gases from the fuel pass out of the upper pipes 10 in the usual manner the cooks 11 being open, which gases are collected and either used to run another retort or stored for future consumption. 1 e

As described in the description of the apparatus, the retort is revolved 180 one or more times during the distillation process, so

former may be removed by opening the top and bottom doors9 of the retort and pushing out the coke from between the horizontal flues 7, leaving the deposit of gas carbon on the tubes and on the inside of the endplates and on the walls of the retort. This retort may be then used where it stands or conveyed away to another portion of the plant by latching the three parts A, B and C together and releasing the bearing around the rods or shafts 17.

The South Carolina clays, which my process is primarily'designed-to treat (although it is by no means restricted to the treatment of these clays) consist of the following parts chemically combined A1' O3,2SiO ,2H,O,

. XFe O that is to say, one molecule of oxidi f sumac of aluminum, two molecules of silica, two 1 molecules of water, and 1 to 3 per cent. of

ferrous or ferric oxide or both, approximately stated.

After determining the amount of alumina in the clay, I mix with one part of clay six times' the amount'of bi-sulfate of sodium, as

. compared with the alumina m the clay, basing the weights aluminum, such as bauxite or corundum.

The quantity of acid bi-sulfate of sodium used should, of course, be suiiicient to furnishwhatever ironis present with a suflicient amount of sulfuric acid, as well asthe alumina, based upon the atomic weights of the oxids of iron and the bi-sulfate of sodiumrvThis mixture is then heated in one of my retortsf roducing a double sulfate of aluminum an sodium re resented by the formula Al (SO 3Na S ferric alum, sulfate of sodium, and free silica, according to the following reaction It should be mentioned that the retort should only be charged "so that it is about twosthirds full and before heating the retort it is separated from the furnace B and chimney connecting portion C and revolved, thus thoroughly mixing the materiaIS together. Then the three parts A B and C are re united, as shown in Fig. 1, and the retort is heated by the furnace B. Sulfuric acid is set free from the bi-sulfate of sodium and attacks the clay, the mass becomes a dark blue color and boils rapidly, and there is a rapid evolution of steam. Ferric alum is formed and also a new compound consistin of a double sulfate of aluminum and so ium, but having 3 molecules of sulfate of sodium combined with 1 molecule of sul- "fate of aluminum. During the same reaction silica is" also formed in an anhydrous condition, and when the reaction is ended, the mass assumes a dirty yellowish white color. As soon as the reaction is ended, the flower bearings 55 e move is rolled of the retort A are removed ap aratus being then free to ofi the track to another portion of the plant. The upper and lower pipes in the retort are ,then opened and steam and the who or hot water is passed in through the pipes at the top and is discharged through the pipes at the bottom, carrying out with, it the contents of the retort. The double sulfates are dissolved out-of.the fused mass,

leaving the silica in an insoluble form. The mass of material obtained by washing out A the retorts is then filtered,

I separating the silica, which is washed again, ,If necessary, and is then in a fine white condition, admirably sulted for making glass poses forv which silica is commonly used.

It will be notedv that by my process the sulfate of aluminum is united chemically with 3 molecules of sulfate of sodiuminstead of with molecule, as in ordinary alum, and by maklng use of this new double sulfate,

and other pur- I have devised an improved sodium process' This double sulfate 18 fused mom of niy retorts with or olite in the proportions indicated by the fbllowing reaction, no carbon being present in the retorts:

sefparated from the solution of the sulfate 0 sodium b filtration. The fluorid of aluminum, .a er being allowed to dry, is heated to about redness and showered down upon melted metallic sodium, whereupon the following reaction takes place:

This reaction results in the roduction of metallic aluminum and cryo ite. At the same time a slag is formed whichmay be used to fuse with the product obtained from clays after fusing them with bi-sulfate of sodium, as mentioned above. x

I obtain metallic sodium as follows: The sulfate of sodium already obtained is placed in one of the retorts A, which has been lined with gas carbon, as previously described. Coke, finely pulverized, may then be added, if necessary, and the retort is then heated till the contents reach a red heat, whereupon sulfid of sodium is-produced, there still being an excess of carbon left in the retort. Caustic lime and more carbon, if needed, are then added and the retort heatedto about 600 C., the heat being finally raised to about 850 C., when metallic sodium commences to distil over and is condensed in the usual manner, the reaction being as follows In other words, I produce metallic sodium indirectly from the sulfate of sodium or directly from the sulfid. I use lime to take the sulfur from the sodium, forming sodium oxid, which is immediately reduced to metallic sodium by the carbon present in the retort. I also manufacturealuminateof sodium, Al O 3Na O, in a similar manner; that is, I place the double sulfate of sodium and aluminum already obtained in one of m carbon lined retorts', and heat it until the manner, which acid is led into a solution of,

sulfate of aluminum is decomposed, formin I silica may be produced, as well as fluorid of aluminum, sulfate of sodiumg,

the 0 id. Sulfurous acid as is driven 0 passes over carbon monoxi and dioxid into a discharge pipe, which leads into a sulfuric acid chamber, where the usual treatment for making sulfuricacid takes place; There is left in'the retort alumina either mixed or' chemically combined with 3 molecules of sulfid ofsodium, Al O 3Na S. I then add caustic lime in suflicient quantities to take up the sulfur, whereupon the following reaction takes place:

The aluminate of sodium thus produced is soluble wlpile the sulfid of calcium is insoluble. The mass is allowed to cool and treated with water, whereupon the aluminate of so dium dissolves and the sulfid of calcium can be separated from the solution byfiltration or decantation.

, Artificial cryolite can also be made from the aluminate of sodium so obtained by treating fiuorid of calcium (fluorspar) in a lead tank with sulfuric acid, whereupon hydro-fluoric acid is formed, in the usual aluminate of sodium through a lead pipe. The following reaction takes place:

The hydro-fluoric acid is rapidly condensed and artificial cryolite is precipitated.

Carbonate of sodium may also be produced as follows: Carbonate of calcium is heated in one of my retorts and the carbonic acid produced is led away and stored up for use. Aluminate of sodium in solution is then treated with this gas, whereu on the hydrate of aluminum is precipitate while carbonate of sodium remains in solution. Whenever carbonates or caustic alkalies are heated at a red heat, the difficulty has been to keep the carbon, which is lighter than the material treated, always in contact with the entire mass of the melted material. In my retort, the gas carbon is fixed around the flues and outer portion of the retort and held there immovably, according to the reactions already set forth. Accordin to my method, a new double sulfate 0 aluminum and sodium, ferric alum, and free series or battery of my retorts without distilling coal in them at all, and in. another series, where it is desirable to use a carbon lined retort, coal is distilled, forming gas and a fresh lining of gas carbon at every distillation, taking care in every distilling operation to tip the retort over, so that the bot-' tom door ison the top and vice versa. The retort is preferably suspended from above by hanging supports, the bottom half bearings being lifted up to the shaft by bolts and screws, as shown in the drawin The retort is detachably fixed to the urnace and chimney connecting portions by means of cylindrical projections fitting into circular grooves, and these with the latches support the retort A when it is 'released from its bearings, so that the whole structure, consisting of the three parts A, Band C may be rolled away to another part of the plant.

I claim:

1. The herein described process of making.

sodium from sodium sulfate, which consists in heating the same with carbon in a closed retort until it is reduced to sodium sulfid;'

then adding calcium oxid to take u the sulfur and to form calcium sulfid, nally raising the temperature to substantially 850 C. and permitting the sodium substantially as described.

In testimony whereof, I afiix my signature,

in presence of two witnesses.

PHILIP I A. EMANUEL.

to distil oif, 

